CN104716322A - Preparation method for modified graphene and application of modified graphene to positive materials for lithium batteries - Google Patents
Preparation method for modified graphene and application of modified graphene to positive materials for lithium batteries Download PDFInfo
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H—ELECTRICITY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of modified graphene and application of the modified graphene to positive materials for lithium batteries. The preparation method for the modified graphene comprises the following steps: preparing a graphene oxide slurry; reducing the graphene oxide slurry at high temperature to prepare graphene; modifying the graphene by a graphene oxidant; modifying the graphene by quaternary ammonium salt; doping the modified graphene into the positive materials for the lithium batteries. The modified graphene prepared by the method has the advantages that the modified graphene is free of agglomeration, excellent in dispersion in solvents, free of toxicity in preparation process, free of pollution to environment and long in service life; through the application of the modified graphene to the positive materials for the lithium batteries, the electric capacity and the charge-discharge rate of the batteries are improved obviously; a small amount of modified graphene is added, so that the cost is reduced.
Description
Technical field
The present invention is specifically related to the preparation method of modified graphene and the application in lithium electricity positive electrode.
Background technology
As a kind of anode material for lithium-ion batteries, LiFePO4 has its relatively high theoretical specific capacity 170mAh/g, has good thermal stability and chemical stability, low cost, hypotoxicity become reconciled security performance, the advantage such as have extended cycle life.But because LiFePO4 exists the low defect of the low and lithium ion conductivity of conductivity, thus cause the poor performance at low temperatures of battery and multiplying power discharging property poor.
Graphene itself is prepared by graphite, and theoretical specific capacity is but 2 times of graphite, (graphite 372mAhg-1, Graphene 744 mAhg
-1).Graphene itself is very thin, wraps up other compounds and forms compound, and can strengthen the invertibity of the discharge and recharge reaction of lithium battery further, application is stronger.But Graphene is easily reunited, cause Graphene dispersive property variation in a solvent, irreversible reunion occurs, causes graphene layer thickness to increase.For this problem, carry out covalent modified to Graphene, solve the problem of reuniting in materials application.
Summary of the invention
In order to overcome the deficiencies in the prior art, solve Graphene in the application easily reunite in problem, the preparation method that a kind of modified graphene is provided of the present invention, the good dispersion of modified graphene prepared by the present invention, be easy to doping process, described modified graphene is used for elements doped lithium electricity positive electrode, obviously can promote capacitance and the charge-discharge magnification of battery.
For achieving the above object, technical scheme is as follows:
The preparation method of modified graphene, comprises the following steps:
A obtains graphene oxide slurry with natural flake graphite and strong oxidizer potassium permanganate, 98% strong sulfuric acid response;
The graphene oxide slurry distilled water obtained cleans to neutrality and dries by b;
C is by the graphene oxide after oven dry, and under high temperature, nitrogen protection, reduction obtains Graphene;
D Graphene joins in oxidizing agent solution ultrasonic, cleaning, dries;
Graphene adds in quaternary ammonium salt solution by e, ultrasonic, suction filtration, vacuum drying, obtains modified graphene product;
Preferably, high temperature described in step c is 400 ~ 1000 DEG C, the Graphene specific area 200 ~ 800m2/g obtained, average grain diameter 15 μm.
Preferably, oxidizing agent solution described in steps d is 30% hydrogen peroxide solution, 10% salpeter solution; The proportioning of described Graphene and oxidizing agent solution is 1g/L ~ 10g/L; Described ultrasonic time is 2 ~ 4h; Described bake out temperature is 60 DEG C.
Preferably, quaternary ammonium salt described in step e comprises at least one in DTAC, tetradecyl trimethyl ammonium chloride, softex kw, OTAC; Described Graphene and quaternary ammonium salt weight ratio are 1:5 ~ 5:1.
Lithium battery positive electrode material containing modified graphene prepared by above-mentioned preparation method, described lithium battery positive electrode material comprises the component of following ratio of weight and number:
Positive electrode 75 ~ 94 parts,
Conductive agent 1 ~ 15 part,
Binding agent 5 ~ 10 parts,
Modified graphene 0.1 ~ 1 part.
Preferably, described modified graphene adds in lithium electricity anode sizing agent, and slurry film is dried, and compressing tablet obtains electrode slice.
Compared to existing technology, the present invention has following beneficial effect:
A. the modified graphene that prepared by the preparation method of modified graphene of the present invention is not reunited, good dispersion in a solvent;
B. the present invention prepares that modified graphene preparation process is nontoxic, pollution-free, the life-span is long;
C. the modified graphene prepared of the present invention is in lithium electricity positive electrode, and the capacitance of battery and charge-discharge magnification obviously promote and addition is few, save cost.
Accompanying drawing explanation
Table 1 for not adding, the battery capacity of Graphene and modified graphene elements doped lithium electricity positive electrode and addition;
Fig. 1 is the SEM figure of modified graphene;
Fig. 2 is the SEM figure of Graphene elements doped lithium electricity positive electrode;
Fig. 3 is the SEM figure of modified graphene elements doped lithium electricity positive electrode.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further illustrated, and raw material of the present invention is all obtained by commercial sources, and preparation method of the present invention is this area customary preparation methods if no special instructions.
embodiment 1
Prepare modified graphene:
(1) graphene oxide slurry is obtained with natural flake graphite and strong oxidizer potassium permanganate, 98% strong sulfuric acid response;
(2) take the graphene oxide slurry of above-mentioned preparation, distilled water cleans to neutrality and dries;
(3) by the graphene oxide after oven dry, 400 DEG C, under nitrogen protection, reduction obtains Graphene;
(4) Graphene ultrasonic 2h in the hydrogen peroxide of oxidant 30%, the proportioning of Graphene and hydrogen peroxide solution is 1g/L, cleans and dries after taking out;
(5) softex kw of compound concentration 0.5mg/mL;
(6) be that Graphene adds in softex kw solution by 1:5 according to Graphene and softex kw mass ratio, after ultrasonic, suction filtration, the oven dry of 60 DEG C, vacuum, obtains sample;
(7) surveying its powder resistivity is 9.70S/cm.
The anode material of lithium battery of preparation containing above-mentioned modified graphene: take modified graphene prepared by 0.1 part of said method, manganate cathode material for lithium 75 parts, conductive agent 1 part, binding agent 5 parts is mixed into uniform sizing material, slurry film is dried, and tabletting machine obtains electrode slice.
embodiment 2
Prepare modified graphene:
(1) graphene oxide slurry is obtained with natural flake graphite and strong oxidizer potassium permanganate, 98% strong sulfuric acid response;
(2) take the graphene oxide slurry of above-mentioned preparation, distilled water cleans to neutrality and dries;
(3) by the graphene oxide after oven dry, 600 DEG C, under nitrogen protection, reduction obtains Graphene;
(4) Graphene ultrasonic 3h in the hydrogen peroxide of oxidant 30%, the proportioning of Graphene and hydrogen peroxide solution is 3g/L, cleans and dries after taking out;
(5) OTAC of compound concentration 0.5mg/mL;
(6) be that Graphene adds in OTAC solution by 2:5 according to Graphene and OTAC mass ratio, after ultrasonic, suction filtration, the oven dry of 60 DEG C, vacuum, obtains sample;
(7) surveying its powder resistivity is 9.70S/cm.
The anode material of lithium battery of preparation containing above-mentioned modified graphene: take modified graphene prepared by 0.3 part of said method, manganate cathode material for lithium 80 parts, conductive agent 3 parts, binding agent 8 parts is mixed into uniform sizing material, slurry film is dried, and tabletting machine obtains electrode slice.
embodiment 3
Prepare modified graphene:
(1) graphene oxide slurry is obtained with natural flake graphite and strong oxidizer potassium permanganate, 98% strong sulfuric acid response;
(2) take the graphene oxide slurry of above-mentioned preparation, distilled water cleans to neutrality and dries;
(3) by the graphene oxide after oven dry, 800 DEG C, under nitrogen protection, reduction obtains Graphene;
(4) Graphene ultrasonic 4h in the salpeter solution of oxidant 10%, the proportioning of Graphene and salpeter solution is 8g/L, cleans and dries after taking out;
(5) tetradecyl trimethyl ammonium chloride of compound concentration 0.5mg/mL;
(6) be that Graphene adds in tetradecyl trimethyl ammonium chloride solution by 2:1 according to Graphene and tetradecyl trimethyl ammonium chloride mass ratio, after ultrasonic, suction filtration, the oven dry of 60 DEG C, vacuum, obtains sample;
(7) surveying its powder resistivity is 12.30S/cm.
The anode material of lithium battery of preparation containing above-mentioned modified graphene: take modified graphene prepared by 0.7 part of said method, manganate cathode material for lithium 90 parts, conductive agent 10 parts, binding agent 9 parts is mixed into uniform sizing material, slurry film is dried, and tabletting machine obtains electrode slice.
embodiment 4
Prepare modified graphene:
(1) graphene oxide slurry is obtained with natural flake graphite and strong oxidizer potassium permanganate, 98% strong sulfuric acid response;
(2) take the graphene oxide slurry of above-mentioned preparation, distilled water cleans to neutrality and dries;
(3) by the graphene oxide after oven dry, 1000 DEG C, under nitrogen protection, reduction obtains Graphene;
(4) Graphene ultrasonic 4h in the salpeter solution of oxidant 10%, the proportioning of Graphene and salpeter solution is clean and dry after 10g/L takes out;
(5) DTAC of compound concentration 0.5mg/mL;
(6) be that Graphene adds in DTAC solution by 5:1 according to Graphene and DTAC mass ratio, after ultrasonic, suction filtration, the oven dry of 60 DEG C, vacuum, obtains sample;
(7) surveying its powder resistivity is 12.30S/cm.
The anode material of lithium battery of preparation containing above-mentioned modified graphene: take modified graphene prepared by 1 part of said method, manganate cathode material for lithium 94 parts, conductive agent 15 parts, binding agent 10 parts is mixed into uniform sizing material, slurry film is dried, and tabletting machine obtains electrode slice.
After adding the modified graphene of this enforcement preparation, lithium battery Contrast on effect data are as table 1 modification elements doped lithium battery Contrast on effect, comparative example 1 is blank test, the common lithium battery that market is sold, comparative example 2 is the Graphene that common lithium battery adds 1% ratio of weight and number, and described Graphene adopts following methods preparation: (1) utilizes the hummer method improved to be obtained by reacting graphene oxide slurry; (2) get a certain amount of graphene oxide slurry, distilled water cleans to neutrality and dries; (3) by the graphene oxide after oven dry, high temperature 400 DEG C, under nitrogen protection, reduction obtains Graphene; (4) the powder conductivity rate surveying its material is 3.08S/cm.Compare as can be seen from Table 1 and the commercially available lithium battery not adding Graphene, after modified graphene prepared by interpolation the present invention, battery capacity obviously increases; Modified graphene prepared by interpolation equivalent weight number Graphene and the present invention, a modified graphene battery capacity increase effect is sent out in the present invention's preparation will obviously be better than commercially available Graphene; The present invention has significant technological progress.Fig. 1 modified graphene SEM picture, the SEM picture of Fig. 2 Graphene elements doped lithium electricity positive electrode, the SEM picture of Fig. 3 modified graphene elements doped lithium electricity positive electrode, modified graphene of the present invention adds to for crystalline state after lithium electricity positive electrode, and crystal grain is conducive to the increase of capacitance and electric power storage, discharge performance.
Table 1
| Material | Capacitance (mAh/g) |
| Comparative example 1 | 110 |
| Comparative example 2 | 120 |
| Embodiment 1 | 126 |
| Embodiment 2 | 130 |
| Embodiment 3 | 136 |
| Embodiment 4 | 131 |
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment to invention has been detailed description, for a person skilled in the art, it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. a preparation method for modified graphene, is characterized in that, the preparation method of described modified graphene comprises the following steps:
Graphene oxide slurry is obtained with natural flake graphite and strong oxidizer potassium permanganate, 98% strong sulfuric acid response;
The graphene oxide slurry distilled water obtained cleaned to neutrality and dry;
By the graphene oxide after oven dry, under high temperature, nitrogen protection, reduction obtains Graphene;
The Graphene of preparation is joined in oxidizing agent solution ultrasonic, cleaning, dry;
Graphene is added in quaternary ammonium salt solution, ultrasonic, suction filtration, vacuum drying, obtain modified graphene product.
2. the preparation method of modified graphene according to claim 1, it is characterized in that, high temperature described in step c is 400 ~ 1000 DEG C.
3. the preparation method of modified graphene according to claim 1, it is characterized in that, oxidizing agent solution described in steps d is 30% hydrogen peroxide solution or 10% salpeter solution; The proportioning of described Graphene and oxidizing agent solution is 1g/L ~ 10g/L; Described ultrasonic time is 2 ~ 4h; Described bake out temperature is 60 DEG C.
4. the preparation method of modified graphene according to claim 1, it is characterized in that, quaternary ammonium salt described in step e comprises at least one in DTAC, tetradecyl trimethyl ammonium chloride, softex kw, OTAC; Described Graphene and quaternary ammonium salt weight ratio are 1:5 ~ 5:1.
5. contain the lithium battery positive electrode material of modified graphene prepared by preparation method described in any one of the claims 1 ~ 4, it is characterized in that, described lithium battery positive electrode material comprises the component of following ratio of weight and number:
Positive electrode 75 ~ 94 parts,
Conductive agent 1 ~ 15 part,
Binding agent 5 ~ 10 parts,
Modified graphene 0.1 ~ 1 part.
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Cited By (4)
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| CN106221863A (en) * | 2016-07-07 | 2016-12-14 | 重庆德领科技有限公司 | Modified graphene lubricating oil that a kind of dispersive property is good and preparation method thereof |
| CN106602039A (en) * | 2017-01-23 | 2017-04-26 | 陕西煤业化工技术研究院有限责任公司 | Functionalized graphene doped nickel cobalt lithium manganate composite cathode material and preparation method thereof |
| CN109830681A (en) * | 2019-01-29 | 2019-05-31 | 中南大学 | A method of improving graphite oxide base anode material capacity |
| CN117343096A (en) * | 2023-12-04 | 2024-01-05 | 瑞浦兰钧能源股份有限公司 | Ionized conductive agent and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117343096A (en) * | 2023-12-04 | 2024-01-05 | 瑞浦兰钧能源股份有限公司 | Ionized conductive agent and preparation method and application thereof |
| CN117343096B (en) * | 2023-12-04 | 2024-04-02 | 瑞浦兰钧能源股份有限公司 | Ionized conductive agent and preparation method and application thereof |
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Application publication date: 20150617 |